CN106521159A - Method for extracting lithium in brine based on extraction system containing Fe (III) and recycling Fe (III) - Google Patents

Method for extracting lithium in brine based on extraction system containing Fe (III) and recycling Fe (III) Download PDF

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Publication number
CN106521159A
CN106521159A CN201610888955.4A CN201610888955A CN106521159A CN 106521159 A CN106521159 A CN 106521159A CN 201610888955 A CN201610888955 A CN 201610888955A CN 106521159 A CN106521159 A CN 106521159A
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iii
extraction
lithium
solution
bittern
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CN106521159B (en
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余晓平
邓天龙
王欢
景妍
李珑
郭亚飞
王士强
王宁军
唐兵
贾晓华
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Tianjin University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a method for extracting lithium in brine based on an extraction system containing Fe (III) and recycling Fe (III). In the process of lithium extraction, the problems that reverse extraction acidity is high, Fe (III) recycling is hard, and the multistage continuous extraction effect is bad exist in a traditional extraction system containing Fe (III). To solve the problems, the method includes the following steps that Fe (III) is loaded in the organic extraction system, and then the lithium in the brine is extracted based on the extraction system containing Fe (III), and NaOH solutions are adopted to conduct reverse extraction on an extracted lithium-rich organic phase. For comprehensive recycling of Fe (III), total Fe (III) is transformed into Fe (OH) 3 and separated, and then transformed into Fe (III) solutions with acid, the Fe (III) solutions are used for the lithium extraction organic phase to be extracted and then recycling of Fe (III) is realized. The method has the advantages that operation is simple, the extraction property of the organic phase is stable, and continuous multistage extraction can be realized, the problems of high acidity and recycling of Fe (III) in the traditional acid reverse extraction process are solved successfully, and application prospects are wide.

Description

Based on lithium and recycling Fe (III) in the extraction bittern of the extraction system containing Fe (III) Method
Technical field
The invention belongs to field of inorganic chemical engineering, is related to a kind of technology of the separation and Extraction lithium from bittern, particularly with regard to A kind of method of lithium and comprehensive reutilization Fe (III) in extraction bittern based on the extraction system containing Fe (III).
Background technology
Lithium is described as " energy metal of 21 century " as important new energy materialses and strategic reserves resource, its exploitation Paid high attention to by the whole world with utilizing.In bittern, lithium reserves account for the 70% of gross reserves, and bittern carries the cost of lithium and scale is excellent Gesture so that the exploitation to lithium resource in bittern become inexorable trend.
Extraction is that lithium extracts a kind of most methods in research in bittern, and studies more for phosphorous organic extraction at present Agent is taken, and tributyl phosphate (TBP) etc. is based particularly on for extractant, FeCl3For synergic reagent, the extractor body that kerosene is diluent System, there is no method to realize commercial Application so far.Trace it to its cause：One is based on containing FeCl3Extraction system extract lithium when, Have that back extraction acidity is high, equipment corrosion is serious, FeCl3The problems such as reclaiming loaded down with trivial details；Two is during traditional extraction, first by FeCl3 It is dissolved in bittern containing lithium, then is extracted with the extraction system based on TBP etc. as extractant, as the system has to Fe (III) There is very high extraction efficiency, when multi-stage counter current extraction is carried out, as major part Fe (III) enters front what extraction in water phase In agent oil phase, cause follow-up series water phase and oil phase in Fe (III) content it is extremely low, so as to not reach multitple extraction purpose (such as Shown in Fig. 1)；Three is the system of organic extraction containing ferric trichloride, and ferric trichloride cannot be realized recycling always.
For the problems referred to above, we develop it is a kind of it is efficiently quick, with low cost, and successfully can solve back extraction acidity and FeCl3The bittern of comprehensive reutilization puies forward lithium method, for the separation and Extraction lithium from bittern and Fe (III) are recycled with weight The commercial Application meaning wanted.
The content of the invention
The purpose of the present invention is for not enough present in art methods, there is provided a kind of extraction based on chloride containing iron The method for taking lithium and comprehensive reutilization Fe (III) in system extraction bittern.
The technical scheme and technical process that the present invention is provided is as follows：
A kind of method of lithium and comprehensive reutilization Fe (III) in extraction bittern based on the extraction system containing Fe (III), its It is characterised by that it comprises the steps：
1) Fe (III) in Fe (III) solution is extracted using the organic extraction system of extraction lithium, separated acquisition The water phase of the Fe containing low concentration (III) after the extractant oil phase containing Fe (III) and extraction.
2) with step 1) middle (III) the organic extraction system containing Fe for obtaining is extracted to lithium in bittern, and separate acquisition After extraction containing Fe (III) water phases and rich lithium oil phase, and according to Na in extracted bittern+、K+、Ca2+、Mg2+Content size, selects Or do not select to wash oil phase after extraction.
3) with NaOH solution to step 2) in rich lithium oil phase carry out back extraction, separated acquisition (OH) containing Fe3Solid phase, back extraction Oil phase afterwards and lithium-containing solution.
4) to step 3) in the lithium-containing solution that obtains after back extraction be evaporated concentration, separate the concentrate Jing coolings after NaCl Crystallization obtains LiCl or and Na2CO3Solution reaction generates Li2CO3, separate LiCl or Li2CO3Rear solution return concentration systems after It is continuous to be evaporated concentration.
5) by step 3) in the oil phase that obtains after back extraction directly return technological process into step 1), or carried out with acid solution Washing, and it is separated wash after oil phase and containing Fe (III) water phase, oil phase returns technological process into step 1), realization The recycling of organic extraction system.
6) by step 1), 2) and 5) in obtain mutually generate individually or with NaOH solution reaction after merging containing Fe (III) water Fe(OH)3Precipitation, and separated acquisition Fe (OH)3Solid phase.
7) by step 3) and the 6) Fe (OH) that obtains3Solid phase generates the solution containing Fe (III) with acid solution reaction, is obtained Fe (III) solution return technological process enter step 1), realize the recycling of Fe (III).
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 1) in extraction organic system be phosphorous organic system, be carried on Fe (III) in organic phase Amount determined according to lithium concentration in extraction phase ratio and bittern, the amount of Fe (III) and selected extraction in be carried on organic phase The ratio for taking the mole for comparing lithium in lower bittern is more than 1:1.
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 2) in extraction phase than O/A (oil phase is than water phase volume) 10:1～1:10 scopes, in extraction Bittern pH=2.0～3.0 are adjusted before taking, and extracting process is single-stage or multi-stage counter current extraction, preferably by multi-stage counter current extraction.
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 3) in back extraction compare O/A 10:1～1:10 scopes, water phase pH≤12 after back extraction, instead Extraction method is single-stage or multi-stage countercurrent back extraction, preferably by multi-stage countercurrent back extraction.
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 4) in concentration after solution in lithium concentration >=5g/L, added Na2CO3Concentration >=5%, Feed way is added to Na for concentrate2CO3Solution, Na2CO3Solution is added to concentrate, both simultaneously additions, it is preferable that dense Contracting liquid is added to Na2CO3Solution, and the process is stirred continuously, charging and reaction time >=5min.
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 5) in institute's acid adding be HCl, H2SO4、HNO3In one or more, it is preferable that use HCl and H+Concentration >=0.01mol/L, washing compare O/A 10:1～1:5 scopes, wash time >=5min.
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 6) in plus NaOH solution reaction after, solution terminal pH is in 4～12 scopes.
And, described one kind is based on lithium and comprehensive reutilization Fe in the extraction bittern of the extraction system containing Fe (III) (III) method, its feature exist：Step 7) in Fe (OH)3The acid of reaction is HCl, H2SO4、HNO3In one or more, Preferably, using dense HCl, and addition is more excessive by 1%～20% than theoretical amount.
Advantages of the present invention and good effect are：
1st, the rich lithium organic phase after the present invention adopts alkaline solution to extraction carries out back extraction, and single back extraction ratio is high, and success Solve etching problem of the sour stripping method middle and high concentration acid to equipment.
2nd, Fe (III) is first extracted and is fixed in extraction organic phase by the present invention, successfully solves Fe (OH)3It is converted into FeCl3Diluting effect of brought into the moisture to bittern in solution processes, and the problem that traditional multi-stage counter current extraction efficiency is low.
3rd, present invention achieves FeCl3Comprehensive cyclic utilization, the process only consumes NaOH and HCl solution, thus cost It is cheap.If additionally, not considering the brine treatment after extracting, the technical process only has the discharge of a small amount of NaCl solution, and Jing suitably locates As chlor-alkali raw material, thus comprehensive utilization of resources and environmental friendliness can be realized after reason.
4th, present invention process realizes the low cost recycling of Fe (III), solves FeCl3Cost and recovery ask Topic, and due to Fe (OH)3Lithium loss problem caused by precipitation.In addition.The method only relates to the extraction of industrial routine, anti- Extraction, precipitation, filtration etc. separate enriching step, simple to operate, it is easy to industrialized production.
Description of the drawings
Fig. 1 is gradually reduced procedure chart for conventional method multitple extraction Fe (III) content；
Fig. 2 is the process chart of the present invention.
Specific embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Lithium in subsurface brine is extracted with process program shown in Fig. 2, bittern consists of Li+、Na+、K+、Ca2+、Mg2+、 Cl-Respectively 0.62,70.9,66.9,26.7,2.6,228.8g/L, additionally containing a small amount of other components.
By FeCl3·6H2O is dissolved in water and adjusts pH<3.0, then extracted with TBP+ sulfonated kerosene systems, contained FeCl containing low concentration after the extractant oil phase of Fe (III) and extraction3Water phase, the FeCl not extracted completely in water phase3Treat back Receive, oil phase is used for extracting lithium.
Adjusted after bittern pH=2.5 with dense HCl, then O/A=2 is being compared with above-mentioned (III) extraction system containing Fe:1 condition Under carry out three-level counter-current extraction, Jing analyses, after three-level counter-current extraction, the extraction yield of lithium is more than 90%.
Separate water phase and oil phase after above-mentioned extraction, FeCl in water phase3To be recycled, rich lithium oil phase is using 0.1mol/L's NaOH is comparing O/A=1:Two grades of back extractions are carried out under the conditions of 1, are centrifuged oil phase, water phase and Fe (OH)3Solid phase.Water is mutually supplied Li is precipitated after concentration2CO3, Jing analyses, the back extraction ratio of lithium up to more than 98% after two grades of back extractions.
HCl solution using 0.05mol/L is comparing O/A=1:Oil phase after back extraction is washed under the conditions of 1, separation is washed Oil phase after washing and contain FeCl3Water phase, oil phase is for recycling, FeCl in water phase3It is to be recycled.
Merge containing FeCl3Water phase, with the NaOH of 0.1mol/L precipitation Fe (III), control terminal pH=8.0, Jing is filtered Separate and obtain Fe (OH)3Solid phase.Obtained solid phase is merged with the solid phase obtained after NaOH back extractions, and it is molten to carry out reaction with dense HCl Solution, the amount of institute enriching HCl are more excessive by 5% than theoretical amount, high concentration FeCl obtained after reaction3Solution lithium organic extractant phase to be extracted is followed Ring is used.
Embodiments of the invention, or the technical scheme of accompanying drawing is had been shown and described above, the excellent of the present invention is embodied Point and efficiently from bittern separation and Extraction lithium and comprehensive reutilization Fe (III) effect.It should be appreciated that being preferable to carry out Example is schematic and nonrestrictive to the detailed description that technical scheme is carried out, and those skilled in the art are reading this On the basis of description of the invention, can be improved according to the above description or be converted, all these modifications and variations should all be belonged to The protection domain of claims of the present invention.

Claims (8)

1. a kind of to be based on the method that the extraction system containing Fe (III) extracts lithium and comprehensive reutilization Fe (III), its feature exists In：Comprise the steps：
1) Fe (III) in Fe (III) solution is extracted using the organic extraction system of extraction lithium, it is separated to obtain containing Fe (III) the water phase of the Fe containing low concentration (III) after extractant oil phase and extraction；
2) with step 1) in (III) the extractant oil phase containing Fe that obtains lithium in bittern is extracted, and after separating and being extracted Containing Fe (III) water phases and rich lithium oil phase, and according to Na in extracted bittern+、K+、Ca2+、Mg2+Content size, to oil after extraction Mutually washed or do not washed；
3) with NaOH solution to step 2) in rich lithium oil phase carry out back extraction, separated acquisition (OH) containing Fe3After solid phase, back extraction Oil phase, lithium-containing solution.
4) to step 3) in the lithium-containing solution that obtains after back extraction be evaporated concentration, separate the concentrate Jing crystallisation by cooling after NaCl Concentrate and Na after obtaining LiCl or separating NaCl2CO3Solution reaction generates Li2CO3, separate LiCl or Li2CO3Solution afterwards Return concentration systems to proceed to be concentrated by evaporation；
5) by step 3) in the oil phase that obtains after back extraction directly return technological process into step 1), or washed with acid solution Wash, and it is separated washed after oil phase and containing Fe (III) water phase, oil phase returns technological process and enters step 1), realized The recycling of machine extraction system；
6) by step 1), 2) and 5) in obtain mutually individually or generate Fe with NaOH solution reaction after merging containing Fe (III) water (OH)3Precipitation, and separated acquisition Fe (OH)3Solid phase；
7) by step 3) and the 6) Fe (OH) that obtains3Solid phase generates the solution containing Fe (III), the Fe for being obtained with acid solution reaction (III) solution returns technological process and enters step 1), realize the recycling of Fe (III).
2. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 1) in organic extraction system be phosphorous organic system, be carried on Fe in organic phase (III) amount determined according to lithium concentration in extraction phase ratio and bittern, in be carried on organic phase the mole of Fe (III) with In bittern, the ratio of the mole of lithium is more than 1:1.
3. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 2) in extraction phase than O/A 10:1～1:10 scopes, adjust bittern before extraction PH=2.0～3.0, extracting process are single-stage or multi-stage counter current extraction.
4. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 3) in back extraction compare O/A 10:1～1:10 scopes, water phase pH after back extraction≤ 12, stripping method is single-stage or multi-stage countercurrent back extraction.
5. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 4) in concentration after solution in lithium concentration >=5g/L, added Na2CO3Concentration >= 5%, feed way is added to Na for concentrate2CO3Solution or Na2CO3Solution is added to concentrate or both while adding, should Process is stirred continuously, and feeds and reaction time >=5min.
6. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 5) in institute's acid adding be HCl, H2SO4、HNO3In one or more of mixture, H+Concentration >=0.01mol/L, washing compare O/A 10:1～1:5 scopes, wash time >=5min.
7. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 6) in plus NaOH solution reaction after, solution terminal pH is in 4～12 scopes.
8. in a kind of extraction bittern based on the extraction system containing Fe (III) according to claim 1, lithium and synthetical recovery are sharp With the method for Fe (III), its feature exists：Step 7) in Fe (OH)3The acid of reaction is HCl, H2SO4、HNO3In one kind or many The mixture planted.
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CN108342595A (en) * 2018-01-26 2018-07-31 天津科技大学 A kind of boron lithium coextraction method in brine
CN110494576A (en) * 2017-03-30 2019-11-22 捷客斯金属株式会社 Lithium recovery method

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